ISO/TC 202 - Microbeam analysis

This document specifies procedures for quantitative analysis of austenite in steel using electron backscatter diffraction (EBSD). This document is mainly applied in low and medium carbon steels, low and medium carbon alloy steels. This document is used to analyse austenite with grain size larger than 50 nm. This method is not used to quantify austenite with grain size smaller than 50 nm, which can significantly affect the accuracy of the analysis results. NOTE 1 The size limit is strongly dependent both on the instrument and the instrument operating parameters. NOTE 2 The size limit is the minimum grain size of the detectable austenite.

This document describes the guidelines for misorientation analysis to assess mechanical damage such as fatigue and creep induced by plastic and/or creep deformation for metallic materials by using electron backscatter diffraction (EBSD) technique. This international standard defines misorientation parameters and specifies measurement conditions for such mechanical damage assessment. This document is recommended to evaluate mechanical damage of austenitic stainless steel, which is widely used for various components of power plants and other facilities. In this document, the mechanical damage refers to the damage which causes the fracture of structural materials due to external overload, fatigue and creep; excepting the chemical and thermal damages themselves.

This document specifies a determination procedure of energy resolution in the scanning transmission electron microscope or the transmission electron microscope equipped with the electron energy loss (EEL) spectrometer. This document is applicable to both in-column type EEL spectrometer and post-column type EEL spectrometer. These EEL signal detecting systems are applicable to a parallel detecting system and a serial detecting system.

This document specifies procedures for quantitative analysis of Mn dendritic segregation in steel billets, blooms, slabs using electron probe microanalysis (EPMA). This document is mainly applicable to continuously cast products with Mn content more than 0,01 % by mass. It can also be used for steel ingots and steel products, such as cast iron and cast steel. The minimum size of analysable dendrites is totally dependent on the resolution of microscope of EPMA and beam size of filament used for quantitative analysis.

This document describes methods to qualify the scanning electron microscope with the digital imaging system for quantitative and qualitative SEM measurements by evaluating essential scanning electron microscope performance parameters to maintain the performance after installation of the instruments. The items and evaluating methods of the performance parameters are selected by users for their own purposes.

This document defines the most important quantities that characterize an energy-dispersive X‑ray spectrometer consisting of a semiconductor detector, a pre-amplifier and a signal-processing unit as the essential parts. This document is only applicable to spectrometers with semiconductor detectors operating on the principle of solid-state ionization. This document specifies minimum requirements and how relevant instrumental performance parameters are to be checked for such spectrometers attached to a scanning electron microscope (SEM) or an electron probe microanalyser (EPMA). The procedure used for the actual analysis is outlined in ISO 22309[2] and ASTM E1508[3] and is outside the scope of this document.

This document describes procedures for measuring average grain size derived from a two-dimensional polished cross-section using electron backscatter diffraction (EBSD). This requires the measurement of orientation, misorientation and pattern quality factor as a function of position in the crystalline specimen[1]. The measurements in this document are made on two dimensional sections. The reader should note carefully the definitions used (3.3) which draw a distinction between the measured sectional grain sizes, and the mean grain size which can be derived from them that relates to the three dimensional grain size. NOTE 1 While conventional methods for grain size determination using optical microscopy are well-established, EBSD methods offer a number of advantages over these techniques, including increased spatial resolution and quantitative description of the orientation of the grains. NOTE 2 The method also lends itself to the measurement of the grain size of complex materials, for example those with a significant duplex content. NOTE 3 The reader is warned to interpret the results with care when attempting to investigate specimens with high levels of deformation.

This document specifies the structure model with related parameters, file format and fitting procedure for characterizing critical dimension (CD) values for wafer and photomask by imaging with a critical dimension scanning electron microscope (CD-SEM) by the model-based library (MBL) method. The method is applicable to linewidth determination for specimen, such as, gate on wafer, photomask, single isolated or dense line feature pattern down to size of 10 nm.

This document specifies specimen preparation methods for the analysis of particles in powders using energy-dispersive spectrometers (EDS) or wavelength-dispersive spectrometers (WDS) installed on an EPMA or SEM. The preparation methods for powder particle analysis are classified by the analytical purpose and the particle size. This document applies to inorganic particles larger than 100 nm and smaller than 100 µm in diameter. It applies only to analysis of "general" powders, which means that it excludes procedures for special applications such as forensic or trace analysis.

This document provides guidelines for performing routine diagnostics and quality assurance procedures on electron probe microanalysers (EPMA). It is intended to be used periodically by an instrument's operator to confirm that the instrument is performing optimally, and to aid in troubleshooting if it is not. It covers the properties of reference materials required and the analysis procedures necessary to independently test and fully evaluate the functionality of the main components of an EPMA system. The analytical procedure described herein is distinct from single-element diagnostic procedures, which can be performed more rapidly. Such procedures are valid for the diffractor position and conditions under which the test is performed, whereas the procedure described herein is intended to qualify an instrument's capabilities for exploratory analysis of unknowns, trace analysis and non-routine work (such as peak interferences). This document is applicable to EPMA and other wavelength dispersive spectrometer (WDS) systems in which elemental identification and quantification are performed by analysis of the energy and intensity of the characteristic X-ray lines observed in wavelength-dispersed X-ray spectra. It is not directly applicable to elemental analysis using energy dispersive spectrometry (EDS).

ISO 25498:2018 specifies the method of selected area electron diffraction (SAED) analysis using a transmission electron microscope (TEM) to analyse thin crystalline specimens. This document applies to test areas of micrometres and sub-micrometres in size. The minimum diameter of the selected area in a specimen which can be analysed by this method is restricted by the spherical aberration coefficient of the objective lens of the microscope and approaches several hundred nanometres for a modern TEM. When the size of an analysed specimen area is smaller than that restriction, this document can also be used for the analysis procedure. But, because of the effect of spherical aberration, some of the diffraction information in the pattern can be generated from outside of the area defined by the selected area aperture. In such cases, the use of microdiffraction (nano-beam diffraction) or convergent beam electron diffraction, where available, might be preferred. ISO 25498:2018 is applicable to the acquisition of SAED patterns from crystalline specimens, indexing the patterns and calibration of the diffraction constant.

ISO 29301:2017 specifies a calibration procedure applicable to images recorded over a wide magnification range in a transmission electron microscope (TEM). The reference materials used for calibration possess a periodic structure, such as a diffraction grating replica, a super-lattice structure of semiconductor or an analysing crystal for X-ray analysis, and a crystal lattice image of carbon, gold or silicon. This document is applicable to the magnification of the TEM image recorded on a photographic film, or an imaging plate, or detected by an image sensor built into a digital camera. This document also refers to the calibration of a scale bar. This document does not apply to the dedicated critical dimension measurement TEM (CD-TEM) and the scanning transmission electron microscope (STEM).

ISO 20263:2017 specifies a procedure for the determination of averaged interface position between two different layered materials recorded in the cross-sectional image of the multi-layered materials. It is not intended to determine the simulated interface of the multi-layered materials expected through the multi-slice simulation (MSS) method. This document is applicable to the cross-sectional images of the multi-layered materials recorded by using a transmission electron microscope (TEM) or a scanning transmission electron microscope (STEM) and the cross-sectional elemental mapping images by using an energy dispersive X-ray spectrometer (EDS) or an electron energy loss spectrometer (EELS). This document is also applicable to the digitized image recorded on an image sensor built into a digital camera, a digital memory set in the PC or an imaging plate and the digitalized image converted from an analogue image recorded on the photographic film by an image scanner.

ISO 19214:2017 prescribes a method for the determination of apparent growth direction by transmission electron microscopy. It is applicable to all kinds of wirelike crystalline materials fabricated by various methods. This document can also guide in ascertaining an axis direction of the second-phase particles with a rod-like or polygonal shape in steels, alloys or other materials. The applicable diameter or width of the crystals to be tested is in the range of tens to hundreds of nanometres, depending on the accelerating voltage of the TEM and the material itself. NOTE In the present document, wirelike crystals, beltlike crystals, needle-shaped second-phase particles, etc. are all subsumed by the broad category of wirelike crystals.

ISO 22489:2016 specifies requirements for the quantification of elements in a micrometre-sized volume of a specimen identified through analysis of the X-rays generated by an electron beam using a wavelength dispersive spectrometer (WDS) fitted either to an electron probe microanalyser or to a scanning electron microscope (SEM). ISO 22489:2016 also describes the following: - the principle of the quantitative analysis; - the general coverage of this technique in terms of elements, mass fractions and reference specimens; - the general requirements for the instrument; - the fundamental procedures involved such as specimen preparation, selection of experimental conditions, the measurements, the analysis of these and the report. ISO 22489:2016 is intended for the quantitative analysis of a flat and homogeneous bulk specimen using a normal incidence beam. It does not specify detailed requirements for either the instruments or the data reduction software. Operators should obtain information such as installation conditions, detailed procedures for operation and specification of the instrument from the makers of any products used.

ISO 16700:2016 specifies a method for calibrating the magnification of images generated by a scanning electron microscope (SEM) using an appropriate reference material. This method is limited to magnifications determined by the available size range of structures in the calibrating reference material. It does not apply to the dedicated critical dimension measurement SEM.

ISO 14594:2014 gives the general guidelines for the determination of experimental parameters relating to the primary beam, the wavelength spectrometer, and the sample that need to be taken into account when carrying out electron probe microanalysis. It also defines procedures for the determination of beam current, current density, dead time, wavelength resolution, background, analysis area, analysis depth, and analysis volume. It is intended for the analysis of a well-polished sample using normal beam incidence, and the parameters obtained can only be indicative for other experimental conditions. It is not designed to be used for energy dispersive X-ray spectroscopy.

ISO 14595:2014 gives recommendations for single-phase certified reference materials (CRMs) used in electron probe microanalysis (EPMA). It also provides guidance on the use of CRMs for the microanalysis of flat, polished specimens. It does not cover organic or biological materials.

ISO 22493:2014 defines terms used in the practice of scanning electron microscopy (SEM). It covers both general and specific concepts, classified according to their hierarchy in a systematic order, with those terms that have already been defined in ISO 23833 also included, where appropriate. ISO 22493:2014is applicable to all standardization documents relevant to the practice of SEM. In addition, some clauses of ISO 22493:2014 are applicable to documents relevant to related fields (e.g. EPMA, AEM, EDS) for the definition of terms which are relevant to such fields.

ISO 17470:2014 gives guidance for the identification of elements and the investigation of the presence of specific elements within a specific volume (on a μm3 scale) contained in a specimen, by analysing X-ray spectra obtained using wavelength dispersive X-ray spectrometers on an electron probe microanalyser or on a scanning electron microscope.

ISO 15932:2013 defines terms used in the practice of AEM. It covers both general and specific concepts classified according to their hierarchy in a systematic order. It is applicable to all standardization documents relevant to the practice of AEM. In addition, some parts of this International Standard are applicable to those documents relevant to the practice of related fields (e.g. TEM, STEM, SEM, EPMA, EDX) for the definition of those terms common to them.

ISO 23833:2013 defines terms used in the practices of electron probe microanalysis (EPMA). It covers both general and specific concepts classified according to their hierarchy in a systematic order. ISO 23833:2013 is applicable to all standardization documents relevant to the practices of EPMA. In addition, some parts of ISO 23833:2013 are applicable to those documents relevant to the practices of related fields (SEM, AEM, EDX, etc.) for definition of those terms common to them.

ISO 22029:2012 presents a simple format for the exchange of digital spectral data that has been designated as an EMSA/MAS standard. This format is readable by both humans and computers and is suitable for transmission through various electronic networks, the phone system (with modems) or on physical computer storage devices (such as removable media). The format is not tied to any one computer, programming language or computer operating system. The adoption of a standard format would enable different laboratories to freely exchange spectral data, and would help to standardize data analysis software. If equipment manufacturers were to support a common format, the microscopy and microanalysis community would avoid duplicated effort in writing data analysis software.

ISO 16592:2012 gives guidance on a method for the determination of the carbon content in steels containing other alloying elements (less than 1 % to 2 % by mass) using the calibration curve method. It specifies the sample preparation, X-ray detection, establishment of the calibration curve and the procedure for the determination of the uncertainty of the measured carbon content. It is applicable to steels containing a mass fraction of carbon of less than 1,0 %. The method is not applicable to steels with higher carbon contents, which could significantly affect the accuracy of the analysis results. ISO 16592 applies to analyses performed using normal beam incidence and wavelength-dispersive X-ray spectrometry; it is not designed to be used for energy-dispersive X-ray spectrometry.

This International Standard provides procedures for electron microprobe elemental-mapping analysis using wavelength-dispersive spectrometry. The choice between mapping with the electron beam moving digitally across the specimen (electron beam mapping) and mapping with stage movement only (large-area mapping) is assessed. It describes five types of data processing: the raw X‑ray intensity data method, the k‑value method, the calibration method, the correlation method and the matrix correction method.

ISO 22309:2011 gives guidance on the quantitative analysis at specific points or areas of a specimen using energy-dispersive spectrometry (EDS) fitted to a scanning electron microscope or an electron probe microanalyser; any expression of amount, i.e. in terms of percent (mass fraction), as large/small or major/minor amounts is deemed to be quantitative. The correct identification of all elements present in the specimen is a necessary part of quantitative analysis and is therefore considered in ISO 22309. ISO 22309 provides guidance on the various approaches and is applicable to routine quantitative analysis of mass fractions down to 1 %, utilizing either reference materials or "standardless" procedures. It can be used with confidence for elements with atomic number Z > 10. Guidance on the analysis of light elements with Z

ISO/TS 24597:2011 specifies methods of evaluating the sharpness of digitized images generated by a scanning electron microscope by means of a Fourier transform method, a contrast-to-gradient method and a derivative method.

ISO 24173:2009 gives advice on how to generate reliable and reproducible crystallographic orientation measurements using electron backscatter diffraction (EBSD). It addresses the requirements for specimen preparation, instrument configuration, instrument calibration and data acquisition.

This International Standard defines the most important quantities that characterize an energy-dispersive X-ray spectrometer consisting of a semiconductor detector, a pre-amplifier and a signal-processing unit as the essential parts. This International Standard is only applicable to spectrometers with semiconductor detectors operating on the principle of solid-state ionization. This International Standard specifies minimum requirements and how relevant instrumental performance parameters are to be checked for such spectrometers attached to a scanning electron microscope (SEM) or an electron probe microanalyser (EPMA). The procedure used for the actual analysis is outlined in ISO 22309[2] and ASTM E1508[3] and is outside the scope of this International Standard.

ISO 29301:2010 specifies a calibration procedure applicable to images recorded over a wide magnification range in a transmission electron microscope (TEM). The reference materials used for calibration possess a periodic structure, such as a diffraction grating replica, a super-lattice structure of semiconductor or an analysing crystal for X-ray analysis, and a crystal lattice image of carbon, gold or silicon. ISO 29301:2010 is applicable to the magnification of the TEM image recorded on a photographic film, or an imaging plate, or detected by an image sensor built into a digital camera. ISO 29301:2010 also refers to the calibration of a scale bar. ISO 29301:2010 does not apply to the dedicated critical dimension measurement TEM (CD-TEM) and the scanning transmission electron microscope (STEM)

ISO 25498:2010 specifies the method of selected-area electron diffraction (SAED) analysis using a transmission electron microscope (TEM) to analyse micrometer and sub-micrometer sized areas of thin crystalline specimens. Such specimens can be obtained in the form of thin sections from a variety of metallic and non-metallic materials, as well as fine powders, or alternatively by the use of extraction replicas. The minimum diameter of the selected area in a specimen which can be analysed by this method depends on the spherical aberration coefficient of the objective lens of the microscope and approaches 0,5 mm for a modern TEM. When the diameter of an analysed specimen area is smaller than 0,5 mm, the analysis procedure can also be referred to ISO 25498:2010 but, because of the effect of spherical aberration, some of the diffraction information in the pattern can be generated from outside of the area defined by the selected-area aperture. In such cases, the use of microdiffraction or convergent beam electron diffraction, where available, might be preferred. The success of the selected-area electron diffraction method relies on the validity of indexing the diffraction patterns arising, irrespective of which axis in the specimen lies parallel to the incident electron beam. Such analysis is therefore aided by specimen tilt and rotation facilities. ISO 25498:2010 is applicable to acquisition of SAED patterns from crystalline specimens, indexing the patterns and calibration of the diffraction constant.

ISO 22493:2008 defines terms used in the practice of scanning electron microscopy (SEM). It covers both general and specific concepts classified according to their hierarchy in a systematic order, with those terms that have already been defined in ISO 23833 also included, where appropriate. The vocabulary is applicable to all standardization documents relevant to the practice of SEM. In addition, some clauses of the vocabulary are applicable to documents relevant to related fields (e.g. EPMA, AEM, EDS) for the definition of terms which are relevant to such fields.

ISO 22489:2006 specifies requirements for the quantification of elements in a micrometre-sized volume of a specimen identified through analysis of the X-rays generated by an electron beam using wavelength-dispersive spectrometers fitted either to an electron probe microanalyser or to a scanning electron microscope. It describes the principle of the quantitative analysis, the general coverage of this technique in terms of elements, mass fractions and reference specimens, the general requirements for the instrument, and the fundamental procedures involved, such as specimen preparation, selection of experimental conditions, the measurements, the analysis of these and the report. It is intended for the quantitative analysis of a flat and homogeneous bulk specimen using a normal incidence beam. It does not specify detailed requirements for either the instruments or the data reduction software. Operators should obtain information such as installation conditions, detailed procedures for operation and specification of the instrument from the makers of any products used.

ISO 16592:2006 gives guidance on a method for the determination of the carbon content in steels containing other alloying elements (less than 1 % to 2 % by mass) using the calibration curve method. It specifies the sample preparation, X-ray detection, establishment of the calibration curve and the procedure for the determination of the uncertainty of the measured carbon content. It is applicable to steels containing a mass fraction of copper of less than 1,0 %. The method is not applicable to steels with higher carbon contents, which could significantly affect the accuracy of the analysis results. ISO 16592:2006 applies to analyses performed using normal beam incidence and wavelength-dispersive X-ray spectrometry; it is not designed to be used for energy-dispersive X-ray spectrometry.

ISO 22309:2006 gives guidance on the quantitative analysis at specific points or areas of a specimen using energy-dispersive spectrometry (EDS) fitted to a scanning electron microscope (SEM) or electron probe microanalyser (EPMA); any expression of amount, i.e. in terms of percent (mass fraction), as large/small or major/minor amounts is deemed to be quantitative. The correct identification of all elements present in the specimen is a necessary part of quantitative analysis and is therefore considered in ISO 22309:2006. ISO 22309:2006 provides guidance on the various approaches and is applicable to routine quantitative analysis of mass fractions down to 1 %, utilising either reference materials or standardless procedures. It can be used with confidence for elements with atomic number Z greater than 10. Guidance on the analysis of light elements with Z less than 11 is also given.

ISO 17470:2004 gives guidance for the identification of elements and the investigation of the presence of specific elements, within a specific volume, contained in a specimen, by analysing X-ray spectra obtained using wavelength dispersive X-ray spectrometers on an electron probe microanalyser or on a scanning electron microscope.

ISO 16700:2004 specifies a method for calibrating the magnification of images generated by a scanning electron microscope (SEM) using an appropriate reference material. This method is limited to magnifications determined by the available size range of structures in the calibrating reference material. This International Standard does not apply to the dedicated critical dimension measurement SEM.

ISO 22029:2003 presents a simple format for the exchange of digital spectral data that has been designated as an EMSA/MAS standard. This format is readable by both humans and computers and is suitable for transmission through various electronic networks (BITNET, ARPANET), the phone system (with modems) or on physical computer storage devices (such as floppy disks). The format is not tied to any one computer, programming language or computer operating system.

ISO 14594:2003 gives the general guidelines for the determination of experimental parameters relating to the primary beam, the wavelength spectrometer and the sample that need to be taken into account when carrying out electron probe microanalysis. It also defines procedures for the determination of beam current, current density, dead time, wavelength resolution, background, analysis area, analysis depth and analysis volume. ISO 14594:2003 is intended for the analysis of a well-polished sample using normal beam incidence, and the parameters obtained may only be indicative for other experimental conditions.

ISO 14595:2003 has been developed to facilitate international exchange and compatibility of analysis data in electron probe microanalysis (EPMA). It gives guidance on evaluating and selecting reference materials (RMs), on evaluating the extent of heterogeneity and stability of RMs and it gives recommendations for the determination of the chemical composition of RMs for production as EPMA certified reference materials. ISO 14595:2003 gives recommendations for single-phase certified reference materials (CRMs) used in electron probe microanalysis (EPMA). It also provides guidance on the use of CRMs for the microanalysis of flat, polished specimens. It does not cover organic or biological materials.

ISO 15632 defines the most important quantities that characterize an energy dispersive X-ray spectrometer (EDS) consisting of a semiconductor detector, a pre-amplifier and a signal processing unit as the essential parts. This International Standard is only applicable to spectrometers with semiconductor detectors operating on the principle of solid state ionization. It specifies minimum requirements for such spectrometers attached to an electron probe microanalyser (EPMA) or a scanning electron microscope (SEM). Realization of the analysis is outside the scope of this International Standard.